US2275558A - Composition for electrical insulation and other technical uses - Google Patents

Description

March 10, 1942. w, c, RODGERS COMPOSITION FOR ELECTRICAL INSULATION AND OTHER TECHNICAL USES 2 Sheets-Sheet 1 Filed June 10, 1938 INVENTOR. WIN/am 6T Foqyers Y fir ATTORNEY V March 10, 1942. w Q RODGERS 2,275,558

COMPOSITION FOR ELECTRICAL INSULATIOfi AND OTHER TECHNICAL USES Fi led June 10, 1938 "2 Sheets-Sheet 2 Z O 3 h 56 =i j 7 56 Y Y XE} F [7 7 62 INVENTOR. C W/Y/I'd fl CI Fad yer;

Patented Mar. 10, 1942 UNITED STATES PATENT OFFICE COMPOSITION FOR ELECTRICAL INSULA- TION AND OTHER TECHNICAL USES William 0. Rodgers, East Orange, N. 1., assignor,

by mesne assignments, to Halowax Corporation, a corporation of Michigan Application June 10, 1938, Serial No. 213,003

Claims.

or fluid state to the solid state and it is also quite noticeable in some compounds if they are permitted to stand in the molten state. The objects of the invention, therefore, are the preparation of solid mixtures of this type which are uniform in composition and which remain uniform in composition when liquefied, and generally to imnaphthalenes, halogenated diphenyls, paraflin wax, halogenated rubber, ceresin, dyes, pigments, bees-wax, etc. Such materials differ widely, both in physical and chemical properties, and skillful blending is required to produce acoating com-' pound of the correct softening point, appropriate viscosity, flexibility and distensibility, freedom from cracking, chipping or crazing, etc. Not only is careful formulation required, but the maintenance of the uniformity and homogeneity of the compound in the course of its application to the conductor is an important desideratum, and has presented a problem which-has heretofore lacked a satisfactory solution in the case of mixtures of materials which stratify. In one aspect, the problem results from the methods commonly used for coating-insulators, which in- .volve melting the wax compounds and then passing the insulator through the molten wax. 'No matter how carefully the compounding of the composition may have been effected, there is always a tendency for one or more of the various components "of the coating compound to segregate when the compound is reduced to the molten state and, as a result, a non-uniform, non-homoductor. Attempts to overcome this by agitating the molten wax have proved unsatisfactory, such agitation having a tendency to introduce air into the compound, and aporous coating is frequently the result.

The problem of producing a uniform and homogeneous coating is aggravated by the fact that many important and useful compounds contain ingredients which attack the rubber or enamel insulation on a wire and these ingredientsalso present certain health hazards. v These are in particular the chlorinated organic compounds which attack rubber and enamel and the vapors of which are prone to give rise to certain skin irritations.

In the actual coating of an electrical conductor of the usual type for instance one having a rubber insulation over the conductor and a fabric covering (that is a covering braided, woven, wound or otherwise constructed of cotton, paper, glass, asbestos, or othertextile or fibrous substances) over the rubber, the conductoris dipped desideratum is as small a bath as possible maintained at as low a temperature as possible yet effective to coat and impregnate the fabric covering. The small bath and low temperature are desirable assuch a bath will give off less fumes than a large bath maintained at a higher temperature. The small bath is also desirable as it is easier to melt at the beginning of the days work after cooling off and solidifying over night and it is easier to bring to a uniform condition after the materials have stratified by standing over night and cooling. But during the working day, it is very much more difficult to maintain uniform conditions in a small bath; than in a large bath particularly where the small bath is maintained at a relatively low temperature. It is impractical to stir a small bath as this introduces air into the bath since the agitator will be quite near the surface of the bath. Furthermore, if the materials added to the bath to make up for those removed by the treated wire are not exceedingly uniform' in composition, the composition of a small bath will change much more than will the composition of a large bath. Also the introduc tion of the materials tends to change the conditions of a small bath much more than a large bath, particularly the temperature of the bath which changes the viscosity and fluidity of the bath and this in turn changes the quantity of coating material absorbed by the fabric, the amount of impregnation of the fabric, the opergeneous coating may be deposited on the conation of the smoothing die, etc. The. effect of only a slight change in temperature is more pronounced where, as in the case of coating compositions containing halogenated materials, the temperature of the bath is maintained as low as possible to prevent fumes and prevent the attack of the rubber by the chemicals and prevent deterioration of the rubber by the heat. With regard to the effect of changes in viscosity, fiuidity and temperatures of the bath, some wires are permitted to remain in the molten bath for only two seconds and consequently the smallest change in the conditions of the bath greatly afiects impregnation of the fabric, and some wires pass through the bath at the rate of approximately 1 feet per second so that the smallest change in the condition of the coating as the wire emerges from the bath and passes through the smoothing die greatly affects the action of the die.

The problems of producing uniform and homogeneous coatings on conductors are more inclusive than merely coating the conductors; these problems extend back to the manufacture of the coating compositions themselves. The compositions as supplied to the wire manufacturer must be uniform and homogeneous and must be in a condition'which facilitates their use by the wire manufacturer to overcome the difiiculties of wire coating as previously pointed out. Also, as previously pointed out, many of these compositions contain halogenated compounds which present certain health hazards during their incorporation into the compositions as the vapors tend to affect a person's skin. Since the compounding of the coating compositions is usually efiected by melting the various ingredients together at elevated. temperatures and with sufficient agitation to give a uniform and homogeneous blend, this has usually necessitated exposing workmen to the ve pors during the mixing, and a definite occupational health hazard results. These molten compounds must then be rapidly cooled; otherwise, the various ingredients often tend to segregate to give a non-uniform, non-homogeneous mass. Since the rapid cooling of large batches is difficult, this has usually necessitated the preparation of relatively small batches of material (for instance 130 lb. lots) or, alternatively, the preparation of large batches of material (for instance 2 to 5 tons) which are subsequently discharged into smaller containers for rapid cooling. Both procedures militate against economical manufacture and involve certain health hazards, since the workmen at some stage in the operations usually are exposed to the vapors of the heated compositions. Moreover, it has been found that even when substantially homogeneous compounds are obtained by vigorous agitation and rapid cooling, such compounds tend to segregate whenthey are maintained in the molten condition for any considerable time.

In the present invention, these difiiculties have been overcome by first compounding the coating ingredients at elevated temperature and then forming the material into individual droplets which harden into small pellets, for instance by subjecting the material to a spray cooling treatment by rapidly ejecting the mixture through a spray nozzle into a cooling chamber. When sprayed, the mixture solidifies in the form of small spherical or oval particles which are easily discharged through a hopper at the bottom of the cooling chamber into suitable containers. The spraying is preferably effected in such a manner that the droplets have a whirling motion during the change from the liquid to the solid state. During this cooling period two phenomena occur: one is that in the case of rather large pellets, say from about 2 /2 to about 5 mm. in diameter which normally take an appreciable time to cool, that is pellets which do not harden until near the bottom of the hereinafter described tower, the materials having the higher specific gravities tend to migrate to the surface of the particles and as the materials which have the highest melting points almost invariably have the highest specific gravities as they densify, the large pellets have an outer shell of the highest melting point material; the second phenomenon is that with smaller pellets say from about /2 to about 2 mm. in diameter which 0001 and harden almost instantaneously throughout the entire mass, the ingredients solidify practically in situ with no appreciable shell or film formation and they show no evidence of segregation of the various ingredients but are exceedingly homogeneous. The shells or films on the larger particles are usually so thin that they can only be noticed under a microscope but they are remarkably efficient in preventing the particles from adhering in a package and they not only prevent the larger particles from adhering but if the smaller particles, in admixture with the larger particles, have a tendency to soften and cause adherence within. the mass of particles, the films or shells form dividing surfaces so that the mass of particles easily separates into individual particles, for instance by a blow from the back of a shovel on a hundred pound sack of the particles.

However, when the particles are used in practical application, for instance when melted to form a wire treating bath or dissolved in lubricating oil for lubricants or milled into rubber, the microscopic film or shell is of negligible effect so far as uniformity of the bath or mixtuie is concerned, and in fact has a beneficial effect. When the particles are melted, the temperature of the bath need be maintained only slightly above the melting point of the'composition since, when a filmed particle is added to the bath, heat passes through the film of high melting point material and liquefies the lower melting point materials in the center of the particle. These lower melting point materials melt at a lower temperature than the temperature of the bath and when in a liquid condition begin to dissolve the film of high melting point material from the inside. Thus the film of high melting point material gets thinner and thinner until finally it is entirely dissolved and the solid pellet has resumed its uniform composition which it had in the original mixing tank; consequently the bath is maintained uniform.

When milled into a plastic material which has rubber-like, elastic properties for instance rubber, neoprene, polyvinyl acetates at elevated temperatures, chlorinated rubber, rubber hydrochloride, hydrogenated rubber, derivatives of polyvinyl acetate, polyvinyl alcohols and their derivatives such as the mixed methylene vinyl acetates, phenol resins in the B state at elevated temperatures, it has been found that these spray cooled particles mix more quickly and easily, and produce a more uniform plastic mixture than do particles of the same size obtained by crushing or grinding the particles from a solid cake. This is believed to be due to the shape and condition of the particles and in the case of those particles which have a hard outer shell to the forces set aa'iaus 3 up within the particle as it cools, particularly in the case of crystalline materials, which tend to shatter the particle when it is ruptured. With particles containing materials which are crystalline in the solid state and more particularly in the case of particles where the outer shell or film of the particle is a crystalline material, crystals begin to form as the pellet begins to cool and as the pellet continues to cool these crystals grow toward the center, the materials which solidify later in the process of cooling the pellet building up on the crystals which have already formed.

Thus when the pellet has entirely solidified, it is a mass of crystals and thereafter when force is exerted on the pellet, for instance when it is milled into rubber, the pellet tends to shatter along the crystal faces formed during the solidi- 'size, there is always the problem of dust which is injurious to the health of the workmen and there is a tendency for ground particles to melt together and agglomerate when put into the oil thus preventing a quick solving at a low temperature. Flaked materials cannot be made in small sizes as can spray cooled materials and they do not dissolve as quickly and 'tend to agfication of the pellet; and thus the plastic conrolls, there is less heat developed and the materials are subjected to heat for a shorter time and thus there is less breakdown of the rubber (and consequently a lighter color which is important in colored wires), less acid develop'ed, less opportunity for the dyes, pigments, or other coloring materials to be affected, etc.

The pelleted materials as described herein present distinct advantages when used as addition agents to lubricating oil. Heretofore solid chlorinated materials such as compounds containing chlorinated naphthalene have been supplied in metallic containers or large cakes from which chunks of the material have been separated. This separation has usually been done with an ax and chips of the material fly from the piece which, together with the use of the ax which is also used to split the metallic containers leaving ragged edges, offer a definite occupational hazard and result in an appreciable loss of material since foreign matter such as dirt, floor sweepings, etc. must be kept out of the oil. Furthermore, when the materials or compounds are formed into cakes or large masses which solidify in the containers, there is a tendency for the stratification to occur so that when chunks are cut off from the main piece, the material as added to the oil may not be uniform. Moreover, when solid chunks of the material (-for instance either a relatively uniform material such as a halogen-' ated naphthalene or a'compound such as one of the chlorinated materials containing another. in-

glomerate. Heat breaks down oil making the oil thinner, produces carbon particles, darkens the color of the oil and reduces its lubricating properties; the heat also has a tendency to break down and adversely affect the majority of addition agents and it is desirable to get the addition agents into the oil as quickly and at as low a temperature as possible.

With the use of pelleted material, however, all of these disadvantages are overcome. The pellets can easily be stirred into and distributed through the oil whereas a chunk cannot and the pellets dissolve much more quickly than a chunk. By adding pellets there is absolute uniformity in the materials added and there are no chips or 1 other occupational hazards. The pellets may be gredient for instance the solid esters, acids, soaps,

etc.) are added to the oil they sink-to the bottom of the mixing tank rather quickly, as their specific gravity is usually greater than that of Also the rounded spray cooled particles can be.

fed to the oil by automatic machinery much more easily than flaked or ground materials as the rounded particles do not adhere to the feeding apparatus. This is particularly noticeable with shelled particles in the portion of the feed device which is adjacent the hot oil and receives both the heat and fumes from the oil. Rounded spray cooled particles will be decidedly more free flowing than will flaked or ground particles and thus the feeding apparatus can be entirely automatic and totally enclosed. The fact that spray cooled particles can be gotten into the lubricating base more quickly and at a lower temperature than large lumps or crushed, ground or flaked material produces a lubricant with a lower and more controllable acid content and better extreme pressure qualities than usual. Thus the advantages of using addition agents as spray cooled particles can readily be understood, these advantages being noticeable in the manufacture of the addition agents, their preparation for and admixture with the oil as well as in the oil composition.

With regard to treating wire, when these'particles are melted to. form a wire treating bath, the uniformity is maintained in the bath, even in the molten state for as much as three hours or longer, thereby enabling the wire manufacturer to overcome the previous difiiculties of a non-uniform melt. Thus, a representative spray cooled material, which had been maintained in a molten condition for about three hours, showed a variation of only 1 C. in flow point throughout the entire mass, whereas a similar material, not spray cooled, when maintained under the same conditions, showed a variation of as much as 6 C.

The spraying operations safeguard the health of the workmen, since the compounding can be done in large enclosed tanks, the fluid mix sprayed into enclosed towers, and the cooled pellets removed without exposing workmen to hazardous vapors.

When fused in a coating bath, the molten pellets not only maintain a uniformity and homogeneity of composition for a time sufliciently long that a uniform coating isdeposited on the conductor, but the pellets permit uniform and controlled additions of the coating composition when it becomes necessary to replenish the coating bath. This is important and advantageous, since it is desirable in wire coating to maintain the coating bath at a temperature only slightly above the softening point of the composition, so that the composition will solidify almost instantly on the emerging wire. Consequently, if the additions of coating compositions can be made at a uniform and controlled rate-say, by feeding a regulated stream of pellets of uniform composition from a hopper--then the temperature of the bath is not abruptly lowered, as would be the case if larger solid fragments of the composition were introduced.

The spray cooled pellets have the further advantage of being dust-free and easy to package. The pellets are easily discharged from the package, since they are rounded in shape and do not readily deform and fuse together under ordinary storage conditions. These characteristics are especially important in comparing these particular pelleted materials with flake materials or h'ollow pellets as these same materials in flake form tend to fuse together and do not feed evenly into a coating bath and in both flake and hollow pellet form tend to produce the dust which is a health hazard and, in addition, the hollow pellets tend to introduce air into the bath. The herein described method of making small particles of these materials is particularly advantageous when the materials are relatively soft, as it is extremely costly or impractical to grind soft, waxy material to obtain small particles. Spray cooling of these materials also produces such a uniform particle size that screening is not required in the majority of cases; if, however, screening is resorted to, the operation is facilitated by the shape of theparticles and can be accomplished more quickly and at a lower cost than with ground material. The dust incident to grinding and screening ground materials is also eliminated which is extremely important in connection with halogenated materials which, in some instances, present health hazards.

In order to more particularly disclose the invention, the process of spray solidifying a representative composition will be disclosed in connection with a suitable apparatus, shown in the accompanying drawings, in which Fig. 1 is a diagrammatic layout of the system.

Fig. 2 is a plan view of the spray tower on the line 22 of Fig. 5.

Fig. 3 is a section through the spray head reservoir.

Fig. 4 is a section through a spray nozzle.

Fig. 5 is a side view of the spray tower.

The apparatus consists generally of a mixing tank 6, a filter press 8, a reservoir l0, pumps I2 and I4, and a cooling tower IS with spray nozzles l8 at the top. 'All parts except the cooling tower are steam jacketed or otherwise heated to maintain the materials in fluid condition and the pumps are used not only to supply the necessary pressure to the material but also to keep the masupplied with a manhole and charging opening 20 at the top and with an agitator 22 to mix the materials thoroughly. From the bottom of the mixing tank, the fluid materials-pass through the pipe line 24 with a cock 26 to the pump l2 which forces the material through the filter press 8 from which it goes to the reservoir in with an agitator 28. From this reservoir the material passes through the pressure and mixing pump M to a spray head reservoir 30 which is also steam jacketed as at 32 with steam inlet and outlet pipes 34 and 36 and from which the spray nozzles I8 deliver the liquefied material to the cooling tower It. The spray nozzles have threaded ends 38 by which they may be screwed into or removed from the spray head reservoir and the inside of the passage is spiralled as at 40 to give the material the whirling motion as it passes through the jet 42. The jet head 44 is removably fastened to the spray nozzle so that jet openings of different sizes may be used and with different angles of spray so that with the various pressures used, the droplets are sprayed in such a direction that they do not impinge upon the side walls 46 of the cooling tower until they'are sufficiently filmed to prevent them from adhering to the walls of the tower. The tower is divided about equally into a conical portion 48 and a cylindrical portion 50. At the bottom of the cylindrical portion are louvers 52 to admit the coolant. These louvers are preferably screened as at 54 to prevent foreign matter from entering the cooling tower and also to prevent small particles of the sprayed materials from escaping into the atmosphere. At the top of the tower are a series of stacks 56, which may be equal in area to or greater or less than the area of the louvers depending upon the draft desired with different compounds and different atmospheric conditions, and preferably with screens 58 permitting the escape of the cooling fluid while holding back any of the particles. The top of the tower is provided with a cover 60 over the spray head reservoir to provide access to the reservoir. At the top of the building 62 there is preferably a ventilating fan 64 which not only ventilates the room in which the cooling chamber is situated but assists in drawing up cooling air over the outer surface of discharging the sprayed material into containers.

terials thoroughly mixed. The mixing tank is This hopper is preferably telescoping with a damper or sluice gate 68.

The molten coating compound may be delivered to the nozzles of the above apparatus at pressures usually from 60-100 lbs. per sq. in. (the higher pressures tending to produce smaller particles) and the size of the nozzle orifices may vary in diameter from 1 mm. to 3 mm. by /2 mm. increments, although nozzle orifices as large as 5, mm. have proved practical. Other pressures may be used depending upon the compound sprayed, the apparatus used and the particle size desired. Too large nozzle orifices are undesirable with the above pressures, as it has been found that with large spherical pellets the previously mentioned advantages of materials in the pellet form tend to disappear, for instance the pellets do not shatter as readily or into as small pieces and they do not melt as quickly, and they also require such a longer time to cool that they are somewhat impractical to manufacture although they can be made with an excessively long cooling chamber and/or a refrigerated coolant.

sprayed is delivered, is of importance andshould,

in general, be as low as possible say only about 20 C.- above the flow point of the material for the above apparatus. If the flow point of the The temperature at which the material to be.

out the length of the sample' .A similar experiment was conducted onmaterial of the same composition and initial flow point as above, but which had been cooled under agitation in a drum. In

material is only a few degrees, say 2 C., above the temperature of the coolant in the apparatus the material may be held at a temperature of only .a' few degrees C. above its flow point, say about 4.

C. If, however, the flow point of the material is in the neighborhoodof 100 C. above the temture'difierence will be necessary, say about 20 6., between the flow point and the: temperature of the material at, which itis held for spraying. The tower into which the material is sprayed is' maintained at a temperature of about 40 C., as a practical matter, using air at room temper-'- ature- Refrigerated coolants may beused to this case, after one hour's heating at 130 C.,

'the flow point varied 3 C. from the flow point of the initial sample, and 4 C. throughout the length of the sample.

In the above example halogenated diphenyl may be used for a part of the halogenated naphthalene and rubber halide or a synthetic resin used for the stearin and jcumar.

' perature of the coolant then a larger tempera- Example 2 the point at which the composition is readily fluid, using wire at room temperature of about 20-25 C. If the wire is preheated to about maintain a lower temperature .ifdesired, havingm mindthat' the pellets should be cooled below. their adhering temperature by the time they reach the conical section-of the'tower or rest on one another. Also the temperatureof'the coolant and the temperatures in the various-portions of the apparatus may becorrelated to the height ofthe apparatus and the cooling time and size of the particles to give particles which are filmed or not and which have large or small crystal formations, as desired. Particles which are well filmed and crystallized are-preferred.

In practical use the rate at which material is delivered to the ,nozzles varies from about 1000 lbs. to 2500 lbs an hour, depending on the viscosity of the material, size of the nozzle orifice,

either of spherical or slightly ovoid shape. Typi- .cal examples of materials which can be sprayed in the manner above described, and the optimum conditions for satisfactory spray cooling are as follows: Example 1 I A mixture of a teristics for instance stearin'pitch 18-to 50 parts, a softening agent whichalso lowers the melting point of the mixture for instance cumar-resin'5 flameprooflng material for instance halogenated naphthalene 50 to 80 parts, a toughening agent with flameprooflng charac-' 100 (2., the bath may beonly 5 to 10 C. above the readily fluid temperature of the materials and if the wire is cold th temperature of the bath may have to be 40 to C. above its readily fluid temperature. A '76 mil. wire with a 12 mil.. rubber insulation and a .25 mil. asbestos covering is passed through the bath at the rate of 1 foot every five seconds and this uses up about 50% of the bath or 20 lbs. of coating composition every hour. By using a constant stream of the herein described spray cooled material, the bath may be maintained uniform in. all ways and evenby introducing the material at the rate of as much as a pound every three minutes they conditions of the bath do not change substantially.

' when the pelleted material is introduced into the number of nozzles, etc. More or less material 1 to 15 parts, an' ingredient to reduce-thetack of the material and resist moisturefor instance 2 to- 20 parts of petroleum wax and dye 1 part, was spray cooled at a pressure of about -70 lbs. and a temperature of about 110-120 C, to give pellets of about 1 mm. in diameter. The resulting spray cooled pellets had flow points of IO-80 C., specific gravities of 1.30-1.40 and 'Stormer viscosities of 10-15 at 130 C. depending upon the particular amounts of materials used. They gave no appreciable evidence of seeregation on being maintained in the molten condition for one hour at 130 C. and were very uniform in'composition, as shown by the following experiment. A particular sampl of spray cooled material (flow point 74 C.) was main- 130" C. and then cooled and sectioned. The flow tained in a 1%" x 12'-' test tube for one hour at bath even so infrequently as 5 lbs. every quarter hour, there is an extraordinary improvement over introducing the same weight of material as a single lump. The pelleted material has a tendency to spread outover the surface of the bath and does not immerse as does a singlelump. Therefore, the pelleted material does not materially change the temperature of the bath and such change as does occur is uniformly distributed. Also the spreading of the particles lessens the surface area from which fumes can e'scape and there is. no deep immersion of solid material to interfere." with free movement of the wire in the bath. In a molten bath of these coating materials two phenomena occur and are utilized to advantage through the use of pelleted material instead of lump material. One of; these is that with the composite materials such as described in the examples, there is a tendency for the material having the greatest vapor pressure to disappear from the molten bath in the vapor form;

the second of these is that the vapors carry with I them their heat of vaporization. Thus when the pelleted materials spread over the surface of the bath, the composition of the bath is maintained more uniform to the extent that the escape of vapors is prevented andthe heat which would ordinarily be lost in the vapors can go into melting the fresh material. As the pellets have been spray cooled and are of uniform composition, the bath is maintained of uniform composition.

From the above, the nature of the problems presented is evident as well as the objects and nature of applicant's invention and the manner 1 in which the problems are solved. The problem point of the material of the various sections was determined and found to vary only about 1 from the initial flow point, and only about V throughof putting a uniform and homogeneous coating on wire, as well as the maintenance of uniform electrical devices, for instance the treatment of coils and particularly the impregnation of condensers, are important in themselves but it will be understood that the invention is of general scope and it is therefore desired that the invention be construed as broadly as the claims taken in conjunction with the prior art may allow.

What is claimed is:

1. Meltable compound which is solid at room temperatures comprising a plurality of ingredients at least one of which is a normally solid, toxic halogenated aromatic hydrocarbon and another of which is a normally solid ingredient of the class consisting of resins, asphalts and waxes, said ingredients being adapted to be melted together to. form a homogeneous fluid mass, the proportions of the ingredients being such that when the mass is in solid condition the ingredients are present beyond their limits of mutual solubility, said compound being in the form of pellets of the solid compound and of substantially uniform composition.

2. Meltable compound which is solid at room temperatures comprising a plurality of ingredients which solidify in the compound at different temperatures, at least one of the ingredients being-a normally solid, toxic halogenated aromatic hydrocarbon and another of the ingredients being a normally solid ingredient of the class of resins, asphalts and waxes, said ingredients being adapted to be melted together to form a homogeneous fluid mass, the proportions of the ingredients being such that when the mass is in solid condition the ingredients are present beyond their limit of mutual solubility, said compound being in the form of pellets of the solid compound and of substantially uniform composition with the ingredient having the highest solidifying temperature as a shell on the outside of the pellets.

3. Method of producing a solid compound containing a plurality of ingredients which are present beyond their limits of mutual solubility but which are distributed substantially uniformly through the compound, one of said ingredients being a normally solid, toxic halogenated aromatic hydrocarbon and another being a normally solid ingredient of the class consisting of resins, asphalts and waxes, which comprises mixing the ingredients in a melted state until a homogeneous mixture is obtained and spraying the melted mixture into a chamber under conditions to produce small particles and solidifying the particles thus sprayed whereby the total mass of the compound has the ingredients substantially uniformly distributed.

4. Method of producing a solid compound containing aplurality of ingredients which solidify in the compound at different temperatures and which are present beyond their limits of mutual solubility but which are distributed substantially uniformly through the compound, one of said ingredients being a normally solid, toxic halogenated aromatic hydrocarbon and another being a normally solid ingredient of the class consisting of resins, asphalts and waxes, which comprises mixing the ingredients in a melted state until a homogeneous mixture is obtained and spraying the melted mixture into a chamber under conditions to produce small whirling liquid particles and solidifying the particles thus sprayed whereby the total mass of the compound has the ingredients substantially uniformly distributed, with the ingredient having the highest solidifying temperature located as a shell on the outside of the solidified particles.

5. Method of producing a solid compound containing a plurality of ingredients one of which has a greater density than another as the compound is cooled from the melted state, said ingredients being present beyond their limits of mutual solubility but distributed substantially uniformly through the compound, one of said ingredients being a normally solid, toxic halogenated aromatic hydrocarbon and another being a normally solid ingredient of the class consisting of resins, asphalts and waxes, which comprises mixing the ingredients in a melted state until a homogeneous mixture is obtained and spraying the melted mixture into a chamber under conditions to produce small whirling liquid particles and solidifying the particles thus sprayed whereby the total mass of the compound has the ingredients substantially uniformly distributed with the ingredient having the said greater density located as a shell on the outside of the solidified particles.

7 WILLIAM C. RODGERS.

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